• 专利标题:   Preparation of hydrogel fibers used in e.g. medical heating detection, involves adding e.g. graphene, cellulose suspension, polyethylene glycol methacrylate and allyl silk fibroin, reacting, squeezing in coagulation bath, and dialyzing.
  • 专利号:   CN112195528-A, CN112195528-B
  • 发明人:   WAN J, WU H, SHUAI L, PENG Z, WANG B
  • 专利权人:   UNIV ZHEJIANG SCITECH
  • 国际专利分类:   C08B015/02, C08F299/02, C08H001/00, D01F001/09, D01F006/52
  • 专利详细信息:   CN112195528-A 08 Jan 2021 D01F-006/52 202113 Pages: 12 Chinese
  • 申请详细信息:   CN112195528-A CN11040734 28 Sep 2020
  • 优先权号:   CN11040734

▎ 摘  要

NOVELTY - Preparation of nanocellulose-reinforced hydrogel fibers involves adding graphene to a cellulose suspension, stirring well and ultrasonically-dispersing to obtain a stable nanocellulose-graphene composite suspension, dissolving polyethylene glycol methacrylate in water to obtain 70-80 mg/mL solution (s1), dissolving allyl silk fibroin, ammonium persulfate and tetramethylethylenediamine in water in an ice water bath, adding to the stable nanocellulose-graphene composite suspension, stirring, introducing a nitrogen gas, dripping into the solution (s1), reacting, transferring to a wet spinning machine, when the solution becomes viscous, squeezing in a coagulation bath at an uniform speed, transferring obtained hydrogel fibers to a dialysis bag, dialyzing using deionized water to remove unreacted substances and drying. USE - Preparation of nanocellulose-reinforced hydrogel fibers used in medical heating detection, monitoring and analysis of human body heat data of smart wearable device and heat source device heating detection. ADVANTAGE - The method enables preparation of nanocellulose-reinforced hydrogel fibers having desired conductivity and temperature sensitivity, and excellent mechanical property. DETAILED DESCRIPTION - Preparation of nanocellulose-reinforced hydrogel fibers involves degumming (i) silkworm cocoons by cutting silkworm cocoons from which pupa is removed, soaking in a boiling sodium carbonate solution, continuously cooking under stirring conditions to remove sericin on surface of cocoons, washing with water, repeating the above processes several times and drying to obtain degummed silk fibers, adding (ii) the silk fibers to 1-butyl-3-methylimidazolium chloride ionic liquid, mixing in a high-speed mixer for 20-40 seconds, stirring and heating at 85-95 degrees C in order to reduce viscosity and melting point of the obtained solution, slowly adding deionized water to the solution to avoid excessive local dilution and cause silk to precipitate out of the solution, centrifuging, when the silk fibers are completely dissolved, transferring the supernatant into a dialysis bag and adding deionized water, in which the mass ratio of silk fibers with respect to deionized water is 1:8-12, dialyzing until water level in the dialysis bag does not change, centrifuging the dialyzed silk fibroin solution in a refrigerated centrifuge, quickly freezing the supernatant and freeze-drying to obtain regenerated silk fibroin, adding (iii) the regenerated silk fibroin to a reaction vessel, dissolving in water, adjusting the pH to alkaline with sodium carbonate and sodium hydroxide, blowing nitrogen, dripping allyl glycidyl ether into the flask while stirring at a constant speed for 15-30 minutes, reacting, adjusting the pH of the solution to neutral with hydrochloric acid solution, placing the reaction solution in a dialysis bag for dialysis, quickly freezing the supernatant and freeze-drying to obtain allyl silk fibroin, dissolving (iv) 0.01-0.02 pt. wt. 2,2,6,6-tetramethylpiperidine-1-oxyl radical and 0.08-0.12 pt. wt. sodium bromide in water, adding 1 pt. wt. bleached wood pulp fibers, stirring vigorously to disperse evenly, adding sodium hypochlorite, oxidizing, controlling the pH of the reaction system at 9.5-10.5 by adding sodium hydroxide solution, filtering the obtained oxidized cellulose, washing with water several times, ultrasonically-dispersing to obtain a slurry having a concentration of 1.5-2.5 mg/mL, stirring in a sealed container and refrigerating to obtain a cellulose suspension, adding (v) graphite powder and a wet medium to a ball milling tank, ball milling, taking out graphene, adding hydrochloric acid to remove excess impurities, washing with deionized water and freeze-drying to obtain graphene, adding (vi) graphene to the cellulose suspension, stirring well and ultrasonically-dispersing to obtain a stable nanocellulose-graphene composite suspension, and dissolving (vii) polyethylene glycol methacrylate in water to obtain 70-80 mg/mL solution (s1), dissolving allyl silk fibroin, ammonium persulfate and tetramethylethylenediamine in water in an ice water bath, adding to the stable nanocellulose-graphene composite suspension, stirring, introducing a nitrogen gas, dripping into the solution (s1), reacting, transferring to a wet spinning machine, when the solution becomes viscous, squeezing in a coagulation bath at an uniform speed, transferring obtained hydrogel fibers to a dialysis bag, dialyzing using deionized water to remove unreacted substances and drying.